KR20210028082A - Aerogel blanket - Google Patents

Abstract

The present invention pertains to an aerogel blanket having a 28-day water impregnation ratio (MIR-28D) of 100 wt% or less as calculated by following equation 1: 28-day water impregnation ratio (MIR-28D, wt%) = {(weight of aerogel blanket after impregnation in 21 ± 2°C distilled water for 28 days - weight of aerogel blanket before impregnation in distilled water) / weight of aerogel blanket before impregnation in distilled water} × 100.

Description

Airgel blanket {AEROGEL BLANKET}

The present invention relates to an airgel blanket, and has excellent long-term water repellency, and relates to an airgel blanket capable of maintaining the thermal insulation performance of the airgel blanket even under severe conditions that may be exposed to moisture for a long period of time.

^{Aerogel is an ultra-porous, high specific surface area (≥500 m 2} /g) material with a porosity of about 90 to 99.9% and a pore size in the range of 1 to 100 nm. Since it is a material having an aerogel material, as well as research on the development of an airgel material, application research as an environmentally friendly high-temperature insulation material, ultra-low dielectric thin film for highly integrated devices, catalysts and catalyst carriers, electrodes for super capacitors, and electrode materials for seawater desalination are actively being conducted.

The biggest advantage of airgel is that it is super-insulation, which has a thermal conductivity of 0.300 W/mK or less, which is lower than that of organic insulation materials such as styrofoam, and it can solve the fire vulnerability, which is the fatal weakness of organic insulation materials, and the generation of harmful gases in case of fire. Is that there is.

In general, airgels are manufactured by preparing a hydrogel from silica precursors such as water glass and alkoxysilane series (TEOS, TMOS, MTMS, etc.), and removing liquid components inside the hydrogel without destroying the microstructure.

In particular, a hydrophobic silica airgel blanket in which a hydrophobic silica aerogel is formed in a fiber is widely used in construction or industrial sites as a functional insulating material that prevents corrosion by moisture, and such a hydrophobic silica aerogel blanket is generally used at the stage of preparing a silica sol solution, It is produced through a gelling step, a aging step, a surface modification step, and a drying step.

However, since the surface modification reaction by the surface modification step starts from the outermost part of the airgel, there is a problem that it is difficult to introduce a sufficient amount of the surface modifying agent to the inside of the airgel. This is because under severe conditions in which the airgel is exposed to moisture for a long period of time, moisture eventually penetrates into the airgel, and moisture adsorption occurs due to hydrogen bonding between the hydroxyl group and moisture present on the surface of the airgel, reducing the durability of the aerogel. It causes the performance to deteriorate.

KR10-2012-0070948A

The present invention was devised to solve the problems of the prior art, and in order to prevent corrosion under insulation (CUI) of airgel, it has excellent long-term water repellency, even under severe conditions that may be exposed to moisture for a long time. An object of the present invention is to provide an airgel blanket capable of maintaining the thermal insulation performance of the airgel blanket.

In order to solve the above problems, the present invention provides an airgel blanket having a moisture impregnation rate of 28 days (MIR-28D) calculated by Equation 1 below of 100% by weight or less.

[Equation 1]

Moisture impregnation rate at 28 days (MIR-28D, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2 ℃ for 28 days-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100

The airgel blanket according to the present invention has excellent long-term water repellency, and thus can maintain the thermal insulation performance of the airgel blanket even under severe conditions that may be exposed to moisture for a long time.

The following drawings attached to the present specification illustrate preferred embodiments of the present invention, and serve to further understand the technical idea of the present invention together with the contents of the above-described invention, so the present invention is limited to the matters described in such drawings. It is limited and should not be interpreted.
1 is a perspective view showing an apparatus for manufacturing an airgel blanket according to a second aspect of a method for manufacturing an airgel blanket according to an embodiment of the present invention.

Hereinafter, the present invention will be described in more detail to aid understanding of the present invention.

Terms and words used in the description and claims of the present invention should not be construed as being limited to their usual or dictionary meanings, and the inventors appropriately explain the concept of terms in order to explain their own invention in the best way. Based on the principle that it can be defined, it should be interpreted as a meaning and concept consistent with the technical idea of the present invention.

"Long-term water repellency" as defined in the present invention means the water repellency ability determined from the increase in weight of moisture absorbed by the airgel blanket when the airgel blanket is exposed to a moisture environment for a long period of time. The "long-term" may mean a period of 7 days (168 hours; 1 week) or more, and specifically ISO:16535 (Thermal insulating products for building applications-Determination of long-term water absorption by immersion; Method 2: total immersion) ) It can mean 28 days (672 hours; 4 weeks) as defined in the standard. Accordingly, in the present invention, when the airgel blanket is exposed to a moisture environment for a long time, the water-repellent ability determined from the increase in weight of moisture absorbed by the airgel blanket is calculated by the following equation (1), the moisture impregnation rate of 28 days (MIR-28D ; Moisture Impregnation Rate of 28 days), and the lower the moisture impregnation rate of 28 days, the better the long-term water repellency.

[Equation 1]

Moisture impregnation rate at 28 days (MIR-28D, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2 ℃ for 28 days-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100

In addition, "Mid-term water repellency" as defined in the present invention means the water repellency ability confirmed from the increase in weight of water absorbed by the airgel blanket when the airgel blanket is exposed to a moisture environment for a medium period. The "medium period" may mean a period of 1 day (24 hours) or more and less than 7 days (168 hours; 1 week), and specifically ASTM C1104 (Standard Test Method for Determining the Water Vapor Sorption of Unfaced Mineral Fiber Insulation ) It can mean 96 hours (4 days) as defined in the standard. Accordingly, in the present invention, when the airgel blanket is exposed to a moisture environment for a medium period, the water-repellent ability determined from the weight increase of moisture absorbed by the airgel blanket is calculated by the following equation (2), and the water impregnation rate of 96 hours (MIR- 96H; Moisture Impregnation Rate of 96 hours), and the lower the moisture impregnation rate of 96 hours, the better the water repellency in the medium term.

[Equation 2]

Moisture impregnation rate of 96 hours (MIR-96H, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2℃ for 96 hours-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100

In addition, "Short-term water repellency" as defined in the present invention means the water repellency ability confirmed from the increase in weight of moisture absorbed by the airgel blanket when the airgel blanket is exposed to a moisture environment for a short period of time. The "short term" may mean a period of less than 1 day (24 hours), and specifically, the "short term" is defined in the ASTM C1511 (Standard Test Method for Determining the Water Retention (Repellency) Characteristics of Fibrous Glass Insulation) standard. It can mean 15 minutes (1/4 hour). Accordingly, in the present invention, when the airgel blanket is exposed to a moisture environment for a short period of time, the water-repellent ability determined from the increase in weight of moisture absorbed by the airgel blanket is calculated by the following equation (3). ; Moisture Impregnation Rate of 15 minutes), and the lower the moisture impregnation rate of 15 minutes, the better the short-term water repellency.

[Equation 3]

Moisture impregnation rate of 15 minutes (MIR-15M, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2 ℃ for 15 minutes-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100

As described above, the hydrophobic silica airgel blanket in which the hydrophobic silica airgel is formed in the fiber is widely used in construction or industrial sites as a functional insulating material that prevents corrosion by moisture, and accordingly, excellent insulation is required. In order to maintain thermal insulation, water repellency is required to prevent the penetration of moisture into the airgel. Accordingly, when the airgel blanket is manufactured to exhibit water repellency, a surface modification step of hydrophobically modifying the surface of the airgel to suppress the penetration of moisture into the airgel blanket is performed. Short-term water repellency can be secured by introducing a hydrophobic group to the outer surface. However, since the surface modification reaction by the surface modification step starts from the outermost part of the airgel, there is a problem that it is difficult to introduce a sufficient amount of the surface modifying agent to the inside of the airgel. This is because under severe conditions in which the airgel is exposed to moisture for a long period of time, as well as for a medium period, moisture infiltrates the interior of the aerogel, resulting in moisture adsorption by hydrogen bonding between the hydroxyl groups present on the surface of the aerogel and moisture, thereby enhancing the durability of the aerogel It lowers and becomes the cause of lowering the heat insulation performance.

Accordingly, in the present invention, by uniformly introducing hydrophobic groups not only to the outermost surface of the airgel, but also to the inner surface of the airgel, moisture is prevented from penetrating into the airgel, thereby providing an airgel blanket having excellent long-term water repellency. Specifically, the present invention provides an airgel blanket having excellent short-term water repellency, medium-term water repellency, and long-term water repellency.

According to an embodiment of the present invention, the airgel blanket may have a moisture impregnation rate (MIR-28D) of 28 days calculated by Equation 1 below of 100% by weight or less.

[Equation 1]

Moisture impregnation rate at 28 days (MIR-28D, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2 ℃ for 28 days-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100

The moisture impregnation rate according to Equation 1 represents the increase in weight increased by impregnating the airgel blanket with distilled water for a long period of time, and the hydroxy groups present on the surface of the airgel must be at most 100% by weight or less for 28 days. It can be seen that the durability of the aerogel can be prevented from deteriorating from moisture adsorption due to hydrogen bonding between and moisture. As in the present invention, in order to minimize the moisture impregnation rate of 28 days, it is necessary to uniformly introduce a hydrophobic group not only to the outermost surface of the airgel, but also to the inner surface of the airgel, which will be described later in the method for manufacturing an airgel blanket according to the present invention. Can be implemented from

According to an embodiment of the present invention, the airgel blanket may have a moisture impregnation rate (MIR-28D) of 90% by weight or less, 70% by weight or less, or 50% by weight or less calculated by Equation 1, Within this range, the long-term water repellency of the airgel blanket is excellent, thereby maximizing durability against moisture penetration.

According to an embodiment of the present invention, the airgel blanket may have a water impregnation rate (MIR-96H) of 96 hours calculated by Equation 2 below of 50% by weight or less.

[Equation 2]

Moisture impregnation rate of 96 hours (MIR-96H, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2℃ for 96 hours-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100

The moisture impregnation rate according to Equation 2 represents an increase in weight increased by impregnating distilled water in the airgel blanket for a medium period, and when the moisture impregnation rate for 96 hours is up to 50% by weight or less, it is expressed as Equation 1 above. Like the calculated moisture impregnation rate of 28 days, there is an effect of preventing the durability of the aerogel from deteriorating due to moisture adsorption due to hydrogen bonding between the hydroxyl group and moisture present on the surface of the airgel. As in the present invention, in order to minimize the moisture impregnation rate of 96 hours, it is necessary to uniformly introduce a hydrophobic group not only to the outermost surface of the airgel, but also to the inner surface of the airgel, which will be described later in the method for manufacturing an airgel blanket according to the present invention. Can be implemented from

According to an embodiment of the present invention, the airgel blanket may have a water impregnation rate of 96 hours (MIR-96H) calculated by Equation (2) of 45% by weight or less or 40% by weight or less, within this range. The blanket has an excellent medium-term and long-term water repellency, thus maximizing durability against moisture penetration.

According to an embodiment of the present invention, the airgel blanket may have a moisture impregnation rate (MIR-15M) of 15 minutes calculated by Equation 3 below of 20% by weight or less.

[Equation 3]

Moisture impregnation rate of 15 minutes (MIR-15M, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2 ℃ for 15 minutes-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100

The moisture impregnation rate according to Equation 3 represents an increase in weight increased by impregnating distilled water in the airgel blanket for a short period of time.When the moisture impregnation rate for 15 minutes is up to 20% by weight or less, a hydrophobic group on the outermost surface of the airgel Is sufficiently introduced to have an effect of preventing moisture from penetrating into the airgel blanket in an environment where the airgel blanket is exposed to moisture.

According to an embodiment of the present invention, the airgel blanket has a moisture impregnation rate (MIR-15M) of 15 minutes calculated by Equation 3 above 15% by weight, 10% by weight or less, 5% by weight or less, 3% by weight It may be less than or less than 1.5% by weight, and within this range, the short-term water repellency of the airgel blanket is excellent, so that the prevention of moisture penetration into the airgel is maximized.

According to an embodiment of the present invention, the airgel blanket has a moisture impregnation rate of 28 days calculated by Equation 1 (MIR-28D) and a moisture impregnation rate of 15 minutes calculated by Equation 3 (MIR-15M). This may satisfy Equation 4 below.

[Equation 4]

(MIR-28D)-(MIR-15M) ≤ 100

Equation 4 may be used to check whether the airgel blanket can secure sufficient water repellency from the relationship between the long-term water repellency and the short-term water repellency of the airgel blanket. Specifically, the moisture impregnation rate (MIR-15M) of 15 minutes calculated by Equation 3, which represents the short-term water repellency of the airgel blanket, is low, so that a hydrophobic group is sufficiently introduced into the outermost surface of the airgel to expose the airgel blanket to moisture. Even if it can be seen that it can prevent moisture from penetrating into the airgel blanket in an environment that can be seen, if the airgel blanket is continuously exposed to moisture for a long period of time, it cannot be seen that all moisture can be prevented from penetrating. Therefore, the moisture impregnation rate of 28 days calculated by Equation 1 representing the long-term water repellency compared to the moisture impregnation rate of 15 minutes (MIR-15M) calculated by Equation 3 representing the short-term water repellency of the airgel blanket (MIR- If 28D) increases rapidly, it cannot be considered that the hydrophobic groups are uniformly introduced not only to the outermost surface of the airgel as in the present invention, but also to the inner surface of the airgel. That is, according to an embodiment of the present invention, when the airgel blanket satisfies Equation 4 above, the airgel blanket sufficiently secures short-term water repellency, and at the same time, it prevents hydrogen bonding between the hydroxyl groups present on the surface of the airgel and moisture. There is an effect of preventing the durability of the airgel from deteriorating due to moisture adsorption. As in the present invention, in order to satisfy Equation 4, it is necessary to uniformly introduce a hydrophobic group not only to the outermost surface of the airgel, but also to the inner surface of the airgel, which is implemented from the method of manufacturing an airgel blanket according to the present invention described below. Can be.

According to an embodiment of the present invention, the airgel blanket has a moisture impregnation rate of 28 days calculated by Equation 1 (MIR-28D) and a moisture impregnation rate of 15 minutes calculated by Equation 3 (MIR-15M). The following Equation 5, the following Equation 6, the following Equation 7, the following Equation 8, or the following Equation 9 may be satisfied, in this case, 15 minutes calculated by Equation 3 indicating short-term water repellency The rapid increase in the water impregnation rate (MIR-28D) of 28 days calculated by Equation 1, which represents the long-term water repellency compared to the moisture impregnation rate (MIR-15M), is controlled, so that the short-term water repellency of the airgel blanket and the mid-term water repellency are controlled. Since both the degree and long-term water repellency are excellent, durability against moisture penetration is maximized.

[Equation 5]

1 ≤ (MIR-28D)-(MIR-15M) ≤ 90

[Equation 6]

1 ≤ (MIR-28D)-(MIR-15M) ≤ 80

[Equation 7]

1 ≤ (MIR-28D)-(MIR-15M) ≤ 70

[Equation 8]

1 ≤ (MIR-28D)-(MIR-15M) ≤ 60

[Equation 9]

1 ≤ (MIR-28D)-(MIR-15M) ≤ 50

According to an embodiment of the present invention, the airgel blanket may have a dust generation amount of 3.0% by weight or less calculated by Equation 10 below.

[Equation 10]

Dust generation amount (% by weight) = {(weight of airgel blanket before vibration-weight of airgel blanket after vibration of 18 Hz/6mm)/weight of airgel blanket before vibration occurrence} X 100.

The amount of dust generated by Equation 10 represents the content of dust, which is a light and small airgel powder remaining in the airgel blanket, and the airgel of the airgel blanket is manufactured as a unit, but at the time of manufacture, dust is a light and small airgel powder separately from the airgel unit. Can inevitably be created. Such dust may cause a decrease in workability when constructing an airgel blanket with an insulating material, etc., obstruct a worker's view, or cause a risk of inhalation by a worker, thereby causing a safety problem for the worker. Therefore, according to an embodiment of the present invention, when the amount of dust generated is at most 3.0% by weight or less, it is possible to prevent deterioration of workability due to dust remaining in the airgel blanket, and the effect of securing the safety of workers is also possible. have.

According to an embodiment of the present invention, the airgel blanket may have a dust generation amount calculated by Equation 10 of 2.0% by weight or less, 1.5% by weight or less, 1.0% by weight or less, 0.5% by weight or less, or 0.4% by weight or less. In addition, within this range, the amount of dust generated by the airgel blanket is minimized, thereby maximizing workability and worker safety.

According to an embodiment of the present invention, the airgel blanket may have a thermal conductivity of 30.0 mW/mK or less at room temperature (23±5° C.). Room temperature thermal conductivity is intended to show the thermal insulation properties of the airgel blanket, and when the maximum is 30.0 mW/mK or less, when the airgel blanket is used as an insulation material, there is an effect of securing sufficient thermal insulation properties.

According to an embodiment of the present invention, the airgel blanket may have a thermal conductivity of 25.0 mW/mK or less, or 20.0 mW/mK or less at room temperature (23±5° C.), and the thermal insulation of the airgel blanket may be maximized within this range. There is an effect that can be secured.

According to an embodiment of the present invention, the airgel blanket may include an airgel and a substrate for a blanket, and an airgel may be formed inside and on the surface of the blanket substrate. As a specific example, the airgel blanket may be formed by uniformly forming a large amount of airgel particles inside and on the surface of the blanket substrate.

In addition, according to an embodiment of the present invention, the airgel may include a hydrophobic group on the inner surface of the airgel. As a specific example, the airgel may be that a hydrophobic group is uniformly introduced not only to the outermost surface of the airgel, but also to the inner surface of the airgel, which may be implemented from the method of manufacturing an airgel blanket according to the present invention described below.

According to an embodiment of the present invention, the airgel blanket is useful as an insulation material for aircraft, ships, automobiles, building structures, heat insulation materials, or non-combustible materials, as well as plant facilities for thermal insulation such as pipes or industrial furnaces of various industrial facilities. Can be used.

In addition, the present invention provides an airgel blanket manufacturing method for manufacturing the airgel blanket.

In order to manufacture the airgel blanket according to the present invention, a manufacturing step for uniformly introducing a hydrophobic group to the inner surface of the airgel as well as the outermost surface of the airgel must be necessarily accompanied. Accordingly, in the present invention, a method of manufacturing an airgel blanket essentially accompanied by the manufacturing step is provided by dividing into a first aspect and a second aspect.

First aspect of the method for manufacturing an airgel blanket

A first aspect of the method for manufacturing an airgel blanket according to the present invention comprises the steps of: 1) preparing a silica sol; 2) impregnating the silica sol into a substrate for a blanket; And 3) leaving the substrate composite for the silica sol-blanket, wherein the silica sol includes a silica precursor composition and a catalyst composition, and the catalyst composition includes a hydrophobic agent, a base catalyst, water, and an organic solvent. , The base catalyst may be included in an amount of 0.4 parts by weight to 1.0 parts by weight based on 100 parts by weight of the silica sol.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the silica sol may be a precursor capable of finally preparing a silica airgel through a gelation reaction, and a silica precursor composition and a catalyst composition are mixed. It may be manufactured by.

In the first aspect of the method for manufacturing the airgel blanket according to an embodiment of the present invention, the silica precursor composition may include a silica precursor, an organic solvent, and water. At this time, the silica precursor included in the silica precursor composition is a material that enables the airgel to be prepared to contain silica, for example, tetramethyl ortho silicate (TMOS), tetraethyl ortho silicate (tetra ethyl ortho silicate). silicate; TEOS), methyl triethyl ortho silicate, dimethyl diethyl ortho silicate, tetra propyl ortho silicate, tetraisopropyl ortho silicate ( tetra isopropyl ortho silicate), tetra butyl ortho silicate, tetra secondarybutyl ortho silicate, tetra tertiarybutyl ortho silicate, tetrahexyl ortho silicate One or more selected from the group consisting of (tetr ahexyl ortho silicate), tetra cyclohexyl ortho silicate, and tetra dodecyl ortho silicate may be used, and the hydrolyzate of the compounds (pre-hydrolysate) may also be used. In the case of using a prehydrolyzed product, addition of an acid is unnecessary, the hydrolysis process of the silica precursor can be shortened or omitted, and the surface modification effect can be promoted. More specifically, in the case of the present invention, the silica precursor (HTEOS) may be a prehydrolyzed polyethyl silicate.

Here, HTEOS is a prehydrolyzed ethyl polysilicate oligomer material having a wide molecular weight distribution, and the degree of prehydrolysis (degree of hydration) is varied to control physical properties such as gelation time when synthesizing from TEOS monomers in oligomer form. Because it can be applied, it can be easily applied according to the reaction conditions of the user. In addition, it has the advantage of creating reproducible physical properties of the final result.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the silica precursor may be used in an amount such that the content of silica contained in the silica sol is 0.1% to 30%. Not limited. When the content of the silica satisfies the above range, it is preferable in terms of having an improved thermal insulation effect while securing the mechanical properties of the airgel blanket, particularly flexibility, to an excellent level.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the organic solvent may specifically be an alcohol, wherein the alcohol is a monohydric alcohol such as methanol, ethanol, isopropanol, butanol, etc.; Alternatively, it may be a polyhydric alcohol such as glycerol, ethylene glycol, propylene glycol, diethylene glycol, dipropylene glycol, and sorbitol, and any one or a mixture of two or more of them may be used. Among these, in consideration of miscibility with water and airgel, it may be a monohydric alcohol having 1 to 6 carbon atoms such as methanol, ethanol, isopropanol, butanol, etc., such as ethanol. The alcohol (organic solvent) and water as described above can be used in an appropriate amount by a person skilled in the art in consideration of the degree of hydrophobicity in the finally produced airgel while accelerating the surface modification reaction.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the catalyst composition includes a hydrophobic agent, a base catalyst, water and an organic solvent, and the base catalyst is 0.4 based on 100 parts by weight of the silica sol. It is characterized in that it contains from parts by weight to 1.0 parts by weight.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the catalyst composition may activate a hydrophobic agent included in the catalyst composition by including water together with a hydrophobic agent in the composition, and the hydrophobic agent is As it is activated, aging and surface modification can be performed without using a separate aging solution and a surface modification solution. Here, activation of the hydrophobic agent may mean that a hydrolysis reaction is performed on a functional group other than an alkyl group of the hydrophobic agent, such as an alkoxy group or a halogen group, thereby forming a hydroxyl group (-OH) at the functional group position. When the hydrophobic agent is activated, the reactivity with the -Si-O- functional group forming the network structure in the silica wet gel can be greatly increased.Therefore, the hydrophobic agent and the silica wet gel react without an additional catalyst and solvent to strengthen the structure and surface. Modification can take place. In addition, accordingly, there is an effect of improving the long-term water repellency of the airgel blanket.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, when a hydrophobic agent is included in the catalyst composition and water is not included, the hydrophobic agent cannot be activated, so subsequent aging and surface modification are performed. In order to do so, it is necessary to perform the aging and surface modification process requiring a large amount of solvent under high temperature conditions as in the conventional method, and even if left under room temperature conditions, there may be a problem that the aging and surface modification reactions do not proceed. Accordingly, since structural reinforcement is not performed, shrinkage of the gel structure may occur during drying, and there may be a problem in that a hydrophobic silica airgel blanket cannot be manufactured due to the absence of a surface modification reaction.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, by using an alkyl silane compound as the hydrophobic agent, the hydrophobic agent may participate in the gelation reaction as a co-precursor, and formed The silica wet gel blanket can be hydrophobized. The alkyl silane compound is gelled with the silica precursor in the gelation step, or the alkyl silane compound contained in the gel undergoes aging and surface modification in the standing step to form an alkyl-Si-O-Si networking to hydrophobize the silica wet gel blanket. When manufacturing the airgel blanket, the surface modification step can be omitted. As a result, it is possible to reduce the amount of the organic solvent and the surface modifier used in the surface modification step, and reduce the process time and manufacturing cost. In addition, the amount of ammonia generated when the surface of the silica wet gel is modified can be greatly reduced, so that the efficiency of reuse of the waste liquid generated after the manufacture of the silica airgel blanket can be increased. Since it can be included in the sol, the amount of the hydrophobic agent used can be greatly reduced by reuse.

Here, the hydrophobic agent may specifically be an alkyl silane compound as described above, and if it is an alkyl silane compound containing an alkyl group inducing hydrophobicization and a silane functional group capable of reacting with the -Si-O-functional group of the wet gel Is not limited, but more specifically trimethylethoxysilane (TMES), trimethylsilanol (TMS), trimethylchlorosilane (TMCS), methyltrimethoxysilane (MTMS), methyltriethoxysilane It may include at least one selected from the group consisting of (MTES), dimethyldiethoxysilane (DMDEOS), ethyltriethoxysilane, and phenyltriethoxysilane.

In addition, in the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, it may be more preferable that the hydrophobic agent does not contain a silazane-based compound such as hexamethyldisilazane. When a silazane-based compound is included, the silazane-based compound may start to decompose when contacted with an organic solvent to generate ammonia, so that a high pH due to the generation of ammonia is formed immediately upon introduction into the catalyst composition containing an organic solvent. The gelling reaction can proceed immediately. Therefore, it is preferable not to include a silazane-based compound from the viewpoint of preventing unexpected gelation reaction and easily controlling the gelation time by changing the amount of catalyst.

In addition, in the first aspect of the method for manufacturing the airgel blanket according to an embodiment of the present invention, the hydrophobic agent is 3 to 15 parts by weight, specifically 5 to 10 parts by weight, more specifically, based on 100 parts by weight of the silica sol. It may contain 6 to 8 parts by weight. Within the above range, the hydrophobicization efficiency (surface modification efficiency) relative to the amount used may be further improved.

In addition, in the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the catalyst composition may contain 3 to 8 equivalents of water based on 1 equivalent of the hydrophobic agent. Specifically, the water may contain 4 equivalents to 8 equivalents, more preferably 5 to 6 equivalents based on 1 equivalent of the hydrophobic agent. When the water contains 3 equivalents or more based on 1 equivalent of the hydrophobic agent, the hydrophobic agent can be sufficiently activated, so that the structure reinforcement and surface modification of the wet gel can easily proceed without an additional catalyst, a surface modifier, and a solvent. It is preferable because a silica airgel blanket having excellent hydrophobicity can be produced without performing a separate surface modification process and wet aging requiring a temperature condition of and a large amount of an organic solvent and a surface modifier. In addition, when the water is contained in an amount of 8 equivalents or less based on 1 equivalent of the hydrophobic agent, the amount of water in the wet gel blanket can be controlled, and accordingly, water is effectively removed during the supercritical drying process to prevent contraction of the airgel by water. As it can be suppressed, thermal conductivity and hydrophobicity can be further improved.

In addition, in the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the base catalyst is included in a range of 0.4 parts by weight to 1.0 parts by weight based on 100 parts by weight of the total silica sol based on 100 parts by weight of the catalyst composition. It may be, and specifically 0.6 parts by weight to 1.0 parts by weight, more specifically 0.6 parts by weight to 0.8 parts by weight may be included. If the base catalyst is contained in an amount of less than 0.4 parts by weight, the reactivity between the hydrophobic agent and the silica gel surface may be weak in the process of standing in step 3), which may cause a problem in that surface modification is not performed. Since the gelation rate is too fast, it is difficult to prepare a uniform gel, and there may be a problem of deterioration of physical properties due to the formation of a non-uniform gel.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the base catalyst may be used without limitation as long as it is a material capable of forming a pH condition so that gelation can be performed, such as sodium hydroxide or hydroxide. Inorganic bases such as potassium; Or an organic base such as ammonium hydroxide.

Specifically, the organic base is ammonium hydroxide (NH ₄ OH), tetramethylammonium hydroxide (TMAH), tetraethylammonium hydroxide (TEAH), tetrapropylammonium hydroxide (TPAH), tetrabutylammonium hydroxide. (TBAH), methylamine, ethylamine, isopropylamine, monoisopropylamine, diethylamine, diisopropylamine, dibutylamine, trimethylamine, triethylamine, triisopropylamine, tributylamine, choline, Monoethanolamine, diethanolamine, 2-aminoethanol, 2-(ethylamino)ethanol, 2-(methylamino)ethanol, N-methyl diethanolamine, dimethylaminoethanol, diethylaminoethanol, nitrilotriethanol, 2 -(2-aminoethoxy)ethanol, 1-amino-2-propanol, triethanolamine, monopropanolamine, or dibutanolamine, and the like, and a mixture of two or more may be used. More specifically, the base catalyst may be ammonium hydroxide (aqueous ammonia; NH ₄ OH).

In addition, in the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the organic solvent is as described above, and the amount of the organic solvent is compatible with water and wet gel, strengthens the structure, and modifies the surface. It can be adjusted appropriately in consideration of ease of use.

In addition, in the first aspect of the method for manufacturing the airgel blanket according to an embodiment of the present invention, the catalyst composition may be included in an amount such that the pH of the silica sol is 4 to 8. When the pH of the silica sol is included to satisfy the above range, gelation may be easily performed and may be performed efficiently. In addition, since the catalyst composition is added in the form of a solution in which a base catalyst is diluted in water and an organic solvent, it is possible to prevent a problem in which the catalyst is precipitated.

The method for manufacturing an airgel blanket according to the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention includes the steps of: 1) preparing a silica sol; 2) impregnating the silica sol into a substrate for a blanket; And 3) leaving the substrate composite for the silica sol-blanket, wherein the silica sol is the aforementioned silica sol.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, step 1) is a step of preparing a silica sol, and may be performed by mixing a silica precursor composition and a catalyst composition. At this time, the silica sol, the silica precursor composition, and the catalyst composition are all as described above. In addition, mixing of the silica precursor composition and the catalyst composition may be performed under conditions of room temperature and pressure.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, by preparing the silica sol described above in step 1), the silica sol-blanket substrate composite is added to the base catalyst in step 3), which will be described later, It is characterized in that gelation, structural reinforcement, and surface modification can be performed even if left without a surface modifier and an organic solvent.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, step 2) is a step of forming a silica sol-blanket substrate composite, wherein the silica sol of step 1) is impregnated into the blanket substrate. It may be done by doing.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the substrate for the blanket may be specifically a porous substrate in terms of improving the thermal insulation properties of the silica airgel blanket. When a porous blanket substrate is used, the silica sol can easily penetrate into the substrate, thereby uniformly forming an aerogel inside the blanket substrate, so that the manufactured silica airgel blanket can have excellent thermal insulation properties.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the blanket substrate may be a film, sheet, net, fiber, porous material, foam, nonwoven fabric, or a laminate of two or more layers thereof. In addition, depending on the use, the surface roughness may be formed or patterned on the surface. Specifically, the blanket substrate may be a fiber capable of further improving thermal insulation performance by including a space or void in which the airgel is easily formed in the blanket substrate, and a material having a low thermal conductivity may be used.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the blanket substrate is polyamide, polybenzimidazole, polyaramid, acrylic resin, phenol resin, polyester, polyether ether ketone (PEEK ), polyolefin (polyethylene, polypropylene, or a copolymer thereof), cellulose, carbon, cotton, wool, hemp, non-woven fabric, glass fiber, or ceramic wool.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, step 3) is a step of leaving the silica sol-blanket substrate composite, wherein gelation, aging, and surface modification are performed in step 3). Can be done.

In addition, in the first aspect of the method for manufacturing the airgel blanket according to an embodiment of the present invention, by using the silica sol of step 1), a separate surface modification solution and a aging solution (base catalyst and solvent) are not used. It is characterized in that the aging and surface modification can be easily performed after gelation without. In this way, since wet aging and a surface modification process using a separate surface modification solution are not performed, the amount of solvent and surface modifier can be significantly reduced compared to the conventional silica airgel blanket manufacturing process. Since the amount of ammonia generated in the base catalyst component included in the aging and the surface modification reaction can be remarkably reduced, the amount of ammonia in the waste liquid generated after manufacturing the airgel blanket can be reduced, thereby increasing the reuse efficiency of the waste liquid. In addition, accordingly, there is an effect of improving the long-term water repellency of the airgel blanket.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, step 3) may be performed under room temperature conditions, and aging and surface modification may be made more easily under the above temperature conditions. . In addition, the room temperature may specifically represent a temperature of 15 to 30 °C, or 15 to 25 °C. In addition, step 3) may be performed for 5 to 48 hours, preferably 10 to 38 hours, more preferably 15 to 24 hours.

In addition, in the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, by adjusting the amount of the base catalyst in the catalyst composition, the gelation time can also be easily adjusted to prepare a silica aerogel of intended physical properties. have. At this time, the preferred gelation time can be adjusted to 1 to 25 minutes, specifically 5 to 10 minutes.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, gelation may be to form a network structure from a precursor material, and the network structure has one atomic arrangement. Alternatively, it may represent a structure in the form of a flat mesh in which certain polygons of a higher type are connected, or a structure that forms a three-dimensional skeleton structure by sharing the vertices, edges, and faces of a specific polyhedron.

In addition, in the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, a step of drying after step 3) may be further included, and a silica hydrophobic silica airgel is prepared by drying the silica wet gel blanket. can do.

Meanwhile, in the first aspect of the method for manufacturing the airgel blanket according to an embodiment of the present invention, the step of washing before drying may be further performed. The washing removes impurities (sodium ions, unreacted products, by-products, etc.) generated during the _{reaction and residual ammonia, which may react with CO 2} during supercritical drying to generate ammonium carbonate, to obtain a high purity hydrophobic silica airgel. It can be carried out by a dilution process or an exchange process using a non-polar organic solvent.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the drying step may be performed through a process of removing a solvent while maintaining the pore structure of the aged silica gel as it is, and the drying step Can be by supercritical drying. The supercritical drying process may be performed using supercritical carbon dioxide. Carbon dioxide (CO ₂ ) is in a gaseous state at room temperature and pressure, but when it exceeds the limit of a certain temperature and high pressure called the supercritical point, the evaporation process does not occur, and it becomes a critical state in which gas and liquid cannot be distinguished. Carbon dioxide in the state is called supercritical carbon dioxide. Although supercritical carbon dioxide has a molecular density close to that of a liquid, its viscosity is low, it has a property close to that of a gas, has a fast diffusion, high thermal conductivity, high drying efficiency, and can shorten a drying process time.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, in the supercritical drying process, the aged silica gel is put in a supercritical drying reactor, and then liquid CO ₂ is filled therein, A solvent replacement process in which the alcohol solvent _{is substituted with CO 2 is performed.} After that, after raising the temperature to 40°C to 80°C at a constant temperature increase rate, specifically at a rate of 0.1°C/min to 1°C/min, a pressure equal to or higher than the pressure at which carbon dioxide becomes a supercritical state, specifically 100 bar to 170 By maintaining the pressure of the bar, the carbon dioxide is maintained for a certain period of time, specifically, 20 minutes to 1 hour in a supercritical state. In general, carbon dioxide becomes supercritical at a temperature of 31 °C and a pressure of 73.8 bar. Carbon dioxide is maintained at a constant temperature and pressure at a supercritical state for 2 to 12 hours, more specifically for 2 to 6 hours, and then the pressure is gradually removed to complete the supercritical drying process to manufacture an airgel blanket. I can.

In the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, as a result of the drying process as described above, a blanket including a porous silica airgel having nano-sized pores and/or a porous silica airgel is manufactured. Can be. The silica airgel has high hydrophobicity and excellent physical properties, particularly low tap density and high porosity, and the silica airgel-containing blanket including the same has low thermal conductivity and excellent mechanical flexibility.

In addition, in the first aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, a pressing process for adjusting the thickness before or after the drying process and uniformizing the inner structure and surface shape of the blanket, suitable for use A molding process to have a shape or morphology, or a lamination process of laminating a separate functional layer may be further performed.

Second aspect of the method for manufacturing an airgel blanket

A second aspect of the method for manufacturing an airgel blanket according to the present invention includes the steps of: 1) introducing the catalyzed sol and the blanket substrate into a reaction vessel, and impregnating the catalyst with the blanket substrate with the catalyzed sol; And 2) rotating and gelling a substrate for a blanket impregnated with the catalyzed sol, wherein the catalyzed sol includes a silica precursor composition, and the silica precursor composition includes a silicate and tetrahydrophobic group. Including an alkyl silicate, the molar ratio of the silicate including the hydrophobic group and the tetraalkyl silicate may be from 60:40 to 98:2.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, step 1) is a step of preparing to form an airgel blanket, by impregnating the sol catalyzed into the substrate for the blanket, and catalyzing It may be to impregnate the catalyzed sol into the blanket substrate by preparing the prepared sol and introducing the prepared catalyzed sol and the blanket substrate into a reaction vessel.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, step 1) is not particularly limited as long as the substrate for the blanket and the catalyzed sol are added to the reaction vessel. . Specifically, the step 1) is a method of introducing a substrate for blanket into a reaction vessel and then introducing a catalyzed sol, a method of introducing a substrate for blanket after introducing the catalyzed sol into a reaction vessel, and catalyzing a catalyst into the reaction vessel. It may be introduced in any one of the methods of injecting the substrate for the blanket while injecting the sol. Among these, it may be more preferable to introduce the catalyst sol after the blanket substrate is added in view of more uniform impregnation. Specifically, when the blanket substrate is first introduced, a more uniform impregnation may be induced because the blanket substrate can be rotated when the catalyzed sol is introduced.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the impregnation in step 1) may be performed while the substrate for the blanket is rotated as described above. When impregnation is performed while rotating the blanket substrate, the sol catalyzed uniformly contacts all surfaces of the blanket substrate to induce uniform impregnation, which is more preferable.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the catalyzed sol may be prepared by mixing a sol and a base catalyst, and the base catalyst is step 2 by increasing the pH of the sol. ) To promote gelation. In this case, the sol is not limited as long as it is a material capable of forming a porous gel through a sol-gel reaction, and specifically, may include an inorganic sol, an organic sol, or a combination thereof. Inorganic sols may include zirconia, yttrium oxide, hafnia, alumina, titania, ceria, silica, magnesium oxide, calcium oxide, magnesium fluoride, calcium fluoride, and combinations thereof, and the organic sol is polyacrylate, Polyolefin, polystyrene, polyacrylonitrile, polyurethane, polyimide, polyfurfural alcohol, phenol furfuryl alcohol, melamine formaldehyde, resorcinol formaldehyde, cresol formaldehyde, phenol formaldehyde, polyvinyl alcohol dialdehyde, polycylate Anurates, polyacrylamides, various epoxies, agar, agarose, and combinations thereof. In addition, in terms of securing excellent miscibility with the substrate for a blanket, further improving porosity when formed into a gel, and manufacturing an aerogel blanket having low thermal conductivity, preferably the sol may be a silica sol.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the sol includes a sol precursor, water, and an organic solvent, and may be prepared by mixing a sol precursor, water, and an organic solvent. When the catalyzed sol according to an embodiment of the present invention is a catalyzed silica sol, the silica sol catalyzed in step 1) may be prepared by mixing a silica sol and a base catalyst, wherein the silica sol Silver may be prepared by mixing a silica precursor composition, water, and an organic solvent. In addition, the silica sol may be hydrolyzed at a low pH to facilitate gelation, and in this case, an acid catalyst may be used to lower the pH. The silica precursor composition usable for preparing the silica sol may include a silicon-containing alkoxide-based compound, and specifically may include a silicate containing a hydrophobic group and a tetraalkyl silicate.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the silicate containing the hydrophobic group is for imparting hydrophobicity to the airgel without a surface modification step during manufacturing the airgel, and methyltriethoxysilane ( MTES), trimethylethoxysilane (TMES), trimethylsilanol (TMS), methyltrimethoxysilane (MTMS), dimethyldiethoxysilane (DMDEOS), ethyltriethoxysilane (ETES) and phenyltriethoxysilane ( PTES) may be one or more selected from the group consisting of. In the case of including a silicate containing a hydrophobic group in the silica precursor composition as described above, it is possible to omit the surface modification step, thereby eliminating the need for a regeneration process when recycling the solvent, and the hydrophobic group can be evenly introduced from the inside to the outside of the aerogel. Therefore, hydrophobicity is maximized, and water having a large surface tension can be easily pushed out by this, so that normal pressure drying is possible in the subsequent drying step. In addition, accordingly, there is an effect of improving the long-term water repellency of the airgel blanket.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the tetraalkyl silicate is for reinforcing the strength of the airgel and securing thermal insulation performance, and tetramethyl orthosilicate (TMOS). ), tetraethyl orthosilicate (TEOS), tetrapropyl orthosilicate, tetraisopropyl orthosilicate, tetrabutyl orthosilicate, tetrasecondarybutyl or Tetra secondary butyl orthosilicate, tetra tertiary butyl orthosilicate, tetrahexyl orthosilicate, tetracyclohexyl orthosilicate, tetracyclohexyl orthosilicate, tetradodecyl orthosilicate (tetradodecyl orthosilicate) and the like may be a tetraalkyl silicate. Among these, more specifically, the silica precursor according to an embodiment of the present invention may be tetraethyl orthosilicate (TEOS).

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the molar ratio of the silicate containing the hydrophobic group and the tetraalkyl silicate in the silica precursor composition may be 60:40 to 98:2, Within this range, it is possible to maximize the strength and thermal insulation performance of the airgel during supercritical drying. In addition, in the case of drying under atmospheric pressure, the molar ratio of the silicate containing the hydrophobic group and the tetraalkyl silicate in the silica precursor composition may be 85:15 to 98:2, or 90:10 to 98:2, and this range While securing the strength and heat insulation performance of the airgel inside with high efficiency, it is possible to prevent the occurrence of shrinkage during normal pressure drying, thereby preventing the heat insulation performance from deteriorating. _{The silica precursor composition may be used in an amount such that the content of silica (SiO 2} ) contained in the silica sol is 3% by weight to 30% by weight, 5% by weight to 20% by weight, or 6% by weight to 12% by weight. . Within this range, the content of the silica airgel in the final manufactured blanket can be sufficiently secured, so that the desired level of thermal insulation effect can be expected, and the formation of excessive silica aerogels prevents the mechanical properties of the blanket, especially the flexibility, from deteriorating. Can be prevented.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the organic solvent that can be used for manufacturing a sol can be used without limitation as long as it has excellent compatibility with a sol precursor and water, and specifically May be to use a polar organic solvent, more specifically to use an alcohol. Here, the alcohol is specifically a monohydric alcohol such as methanol, ethanol, isopropanol, butanol, and the like; Alternatively, it may be a polyhydric alcohol such as glycerol, ethylene glycol, propylene glycol, diethylene glycol, dipropylene glycol, and sorbitol, and any one or a mixture of two or more of them may be used. Among these, in consideration of miscibility with water and an airgel to be produced in the future, it may be a monohydric alcohol having 1 to 6 carbon atoms such as methanol, ethanol, isopropanol, butanol, and the like. The organic solvent as described above may be used in an appropriate amount in consideration of the content of the finally produced airgel.

In the second aspect of the method for manufacturing the airgel blanket according to an embodiment of the present invention, the silica sol may include a silica precursor composition and water in a molar ratio of 1:10 to 1:1. In addition, the silica precursor composition and the organic solvent may be included in a weight ratio of 1:2 to 1:9, and preferably may be included in a weight ratio of 1:2 to 1:6. When the silica precursor composition satisfies the molar ratio or weight ratio of water and organic solvents, the yield of airgel production may be further increased, and thus there is an improvement effect in terms of thermal insulation performance.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the acid catalyst that may be further included in the sol may be used without limitation as long as the acid catalyst has a pH of 3 or less. For example, hydrochloric acid, Nitric acid or sulfuric acid may be used. In this case, the acid catalyst may be added in an amount such that the pH of the sol is 3 or less, and may be added in the form of an aqueous solution dissolved in an aqueous medium.

In addition, in the second aspect of the method for manufacturing the airgel blanket according to an embodiment of the present invention, the base catalyst usable in the catalyzed sol includes inorganic bases such as sodium hydroxide and potassium hydroxide; Or an organic base such as ammonium hydroxide. Specifically, sodium hydroxide (NaOH), potassium hydroxide (KOH), calcium hydroxide (Ca(OH) ₂ ), ammonia (NH ₃ ), ammonium hydroxide (NH ₄ OH; aqueous ammonia), tetramethylammonium hydroxide (TMAH), tetra Ethyl ammonium hydroxide (TEAH), tetrapropylammonium hydroxide (TPAH), tetrabutylammonium hydroxide (TBAH), methylamine, ethylamine, isopropylamine, monoisopropylamine, diethylamine, diiso Propylamine, dibutylamine, trimethylamine, triethylamine, triisopropylamine, tributylamine, choline, monoethanolamine, diethanolamine, 2-aminoethanol, 2-(ethylamino)ethanol, 2-(methyl Amino) ethanol, N-methyl diethanolamine, dimethylaminoethanol, diethylaminoethanol, nitrilotriethanol, 2-(2-aminoethoxy)ethanol, 1-amino-2-propanol, triethanolamine, monopropanolamine, It may be one or more selected from the group consisting of dibutanolamine and pyridine, preferably sodium hydroxide, ammonia, ammonium hydroxide, or a mixture thereof. The base catalyst may be included in an amount such that the pH of the sol is 7 to 11. If the pH of the sol is out of the above range, gelation in step 2) to be described later is not easy, or the gelation rate is too slow, and thus fairness may be deteriorated. In addition, since the base may be precipitated when introduced into a solid phase, it may be preferably added in the form of an aqueous medium or a solution diluted with the above-described organic solvent. In this case, the dilution ratio of the base catalyst and the organic solvent, specifically alcohol, may be 1:4 to 1:100 on a volume basis.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the catalyzed sol may further add an additive as necessary, and the additive may be added when preparing an aerogel. All of the additives may be applied, for example, additives such as an opacifying agent and a flame retardant may be used. The blanket substrate may be introduced in a suitable shape that is easy to input according to the shape of the reaction vessel, and specifically, a blanket substrate wound in a roll shape on a bobbin to facilitate rotation in step 2) to be described later It may be added to the reaction vessel. In this case, the bobbin may be a shaft capable of rotating the blanket substrate, and any one that can wind the blanket substrate may be applied without limitation. As an example, it may be to use a polygonal cylindrical column, preferably a cylindrical column having a size that can fit inside the reaction vessel.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the bobbin includes a winding rod capable of winding a blanket substrate in a roll form, and a blanket substrate wound around the winding rod does not deviate during rotation. It may include a support plate to support the side to prevent. At this time, it is preferable that there are a number of hollows in the winding rod so that the catalyzed sol is easily impregnated inside the blanket substrate. On the other hand, the support plate may use a mesh type or may include a plurality of hollows so that the sol catalyzed to the side of the blanket substrate can flow. The material of the bobbin may be any material having sufficient strength to support the blanket, and specifically stainless steel, PE, PP, Teflon, etc. may be used.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the bobbin may be a method of wrapping a substrate for a blanket and then putting it into a reaction vessel and fixing it. Here, the bobbin can be fixed at any position of the reaction vessel, but a lot of the blanket substrate is added in the reaction vessel of the same volume, and thus, in terms of increasing production efficiency, the bobbin is preferably fixed to the center of the reaction vessel. Can be. In addition, it may be to position the bobbin so that the long axis of the bobbin and the long axis of the reaction vessel are parallel to each other.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the substrate for the blanket may be specifically a porous substrate in terms of improving the thermal insulation properties of the airgel blanket. When a porous blanket substrate is used, the catalyzed sol easily penetrates into the substrate, and thus the airgel blanket formed uniformly forms the airgel inside the blanket substrate, so that the manufactured airgel blanket can have excellent thermal insulation properties.

The blanket substrate that can be used according to the second aspect of the airgel blanket manufacturing method according to an embodiment of the present invention may be a film, sheet, net, fiber, foam, nonwoven fabric, or a laminate of two or more layers thereof. In addition, depending on the use, the surface roughness may be formed or patterned on the surface. More specifically, the blanket substrate may be a fiber capable of further improving thermal insulation performance by including spaces or voids in which the airgel can be easily inserted into the blanket substrate. In addition, it may be desirable that the blanket substrate has a low thermal conductivity.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the substrate for the blanket is polyamide, polybenzimidazole, polyaramid, acrylic resin, phenol resin, polyester, polyetheretherketone ( PEEK), polyolefin (e.g., polyethylene, polypropylene, or a copolymer thereof), cellulose, carbon, cotton, wool, hemp, non-woven fabric, glass fiber, ceramic wool, etc., and more specifically in the present invention, the The substrate for the blanket may be glass felt (glass fiber).

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the reaction vessel may be a reaction vessel for performing gelation, and the substrate for blanket impregnated with the catalyzed sol may be rotated. Any container of any shape, such as a polygonal cylinder or a cylindrical shape, can be used as long as it forms a space, but it also facilitates the injection of the blanket substrate wound in a roll shape, and the rotation of the blanket substrate impregnated with the catalyst sol during the gelation reaction In terms of this ease of use, a cylindrical reaction vessel can be preferably used.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, when the sol catalyzed in step 1) is introduced, the substrate for a blanket is used to improve the bonding between the substrate for the blanket and the catalytic sol. Press lightly to ensure sufficient impregnation. After that, by pressing the substrate for the blanket to a predetermined thickness with a constant pressure to remove excess sol, it is also possible to reduce the drying time. In another embodiment, when the catalyst is added to the reaction vessel, the blanket substrate is sufficiently impregnated and the remaining sol may be recovered when the liquid level in the reaction vessel is no longer changed. Silver may be recovered by opening a drain valve connected to the reaction vessel.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the catalyst for the sol and blanket is the volume of the reaction vessel, specifically, 1 to 100% of the inner volume of the reaction vessel. Each can be added, and from the viewpoint of shortening the gelation time in step 3) and forming an airgel uniformly inside the blanket substrate, preferably in an amount of 1 to 60% of the volume of the reaction vessel, more preferably 10 to It may be to add an amount of 60%, more preferably 30 to 60%, respectively.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the sol catalyzed based on the volume of the blanket substrate is added in an amount of 80 to 120%, preferably 90 to 110%. can do. In addition, preferably, the amount of the blanket substrate and the catalyzed sol may be one that satisfies the above-mentioned ratio of each other under the condition of satisfying the amount of injection compared to the reaction vessel. When the catalyzed sol satisfies the input ratio (input amount) to the volume of the blanket substrate, the aerogel blanket produced by impregnating the catalyst sol more evenly into the blanket substrate may have more uniform physical properties, and the catalyzed sol Since all of this blanket substrate can be impregnated, loss of raw materials can be prevented and the problem of gelation of the catalyzed sol alone can be prevented.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, step 2) is for preparing a wet gel blanket composite (wet gel blanket), and a substrate for a blanket impregnated with a catalyzed sol is used. It may be performed by rotating and gelling.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, any method and apparatus in which the rotation of the substrate for blanket impregnated with the catalyzed sol is a method of rotating while gelling in a reaction vessel. It can also be used, and specifically, when the blanket substrate is wound around the bobbin in step 1) and fixed, the blanket substrate impregnated with the catalyzed sol is present in the reaction vessel in a state wound around the bobbin. , By rotating the bobbin, the substrate for blanket impregnated with the catalyzed sol may be rotated.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the gelation may be forming a network structure from a catalyzed sol, and the network structure is an atomic arrangement. It may represent a structure in the form of a flat mesh in which a certain polygon of one or more types is connected, or a structure that forms a three-dimensional skeleton structure by sharing the vertices, edges, and faces of a specific polyhedron.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, a gelling reaction may be performed after sealing a reaction vessel in which the catalyzed sol and the substrate for the blanket are added. In addition, according to an embodiment of the present invention, the long axis may be disposed in a transverse direction, that is, in a horizontal direction to rotate. If the reaction vessel (body) is a cylindrical reaction vessel, the cylindrical reaction vessel may be laid down and rotated. That is, the rotation axis of the reaction vessel of the present invention may be in a horizontal direction, but is not limited thereto.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the substrate for a blanket including the reaction vessel (body) and impregnated with the catalyzed sol present in the reaction vessel can be rotated. The type of the airgel blanket manufacturing apparatus is not limited, and any known apparatus may be used as long as it can be rotated. Specifically, any known device may be used as long as the position of the bobbin can be fixed to the reaction vessel and the position of the bobbin is rotated. An example of an apparatus for manufacturing an airgel blanket applicable in the present invention will be described later.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, after the step 1) is completed, the step 2) is initiated, and the step 1) and the step 2) are sequentially performed. It can be done with.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, it may be to initiate and perform step 2) before step 1) is completed, and thus before completion of step 1). In the case of performing step 2), it may be to put all of the catalyzed sol into the reaction vessel until the gelation is completed, specifically before the gelation is completed.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the rotational speed in step 2) can be applied without limitation in terms of rotational speed so that the airgel in the blanket can be uniformly formed, For example, it may be to perform gelation while rotating at a rotational speed of 1 rpm to 300 rpm, preferably 5 rpm to 150 rpm, 5 rpm to 100 rpm, more preferably 10 rpm to 30 rpm. If the reaction vessel satisfies the above range of rotational speed, the sol in the blanket substrate may be evenly impregnated, so that the aerogel is formed more evenly during gelation, and thus, very uniform thermal conductivity can be secured throughout the airgel blanket and the reaction There is an advantage of increasing the safety of the airgel blanket manufacturing process by increasing the stability of the container and the device that rotates it.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, both the catalytic sol and the blanket substrate are put in a reaction vessel and gelled to produce an airgel blanket, so that the conventionally applied roll-to-roll method and In contrast, since moving elements such as a conveyor belt are not required separately, there is an advantage in that the space used during manufacturing can be greatly saved. In addition, as in the roll-to-roll method, when a blanket substrate is placed on a moving element and a catalyzed sol is applied to the blanket substrate to gel while continuing to move the moving element, gelation is performed simultaneously on the entire blanket substrate. The gelling process according to an embodiment of the present invention, even if a blanket substrate having the same thickness and length is used because gelling is inevitable sequentially according to the passage of time while continuously supplying the blanket substrate and the catalyzed sol. A problem occurs that takes significantly longer than that. In particular, the longer the blanket substrate is, the more pronounced the problem of lengthening the gelling process time in order to achieve sufficient gelation throughout the blanket substrate.According to an embodiment of the present invention, gelation of the sol is simultaneously performed in the entire blanket substrate. Because of this, the manufacturing time can be remarkably reduced, and since the length and thickness of the blanket substrate do not affect the gelation time, even if a long blanket substrate is used, the manufacturing time can be significantly reduced, thereby maximizing process efficiency.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the reaction vessel is not rotated or gelled on the moving element because the centrifugal force and the centripetal force act by performing gelation while rotating the reaction vessel. Compared to the roll-to-roll method, it is possible to manufacture an airgel blanket in which the airgel is more uniformly dispersed, so that the thickness of the airgel blanket to be produced is the same or extremely similar to the thickness of the substrate for the blanket, and there is an excellent heat insulation effect.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the wet gel blanket composite may be left at an appropriate temperature to complete a chemical change, and the aging step may be performed, and the aging step The formed network structure can be formed more firmly, it is possible to enhance the mechanical stability of the airgel blanket of the present invention.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the aging step may be carried out by leaving the wet gel blanket composite itself at an appropriate temperature. In the presence of sodium hydroxide (NaOH), potassium hydroxide (KOH), ammonium hydroxide (NH ₄ OH), triethylamine, pyridine, etc. I can. In this case, by inducing Si-O-Si bonding in the airgel to the maximum, the network structure of the silica gel is made more solid, and thus the maintenance of the pore structure in the fast drying process to be performed later is more easily effective. In this case, the organic solvent may be the aforementioned alcohol (polar organic solvent), and specifically, may include ethanol.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the aging step should be performed at an appropriate temperature range for reinforcing the optimal pore structure, but the aging step of the present invention is the introduction of a basic catalyst. Regardless of whether or not, it may be performed by allowing it to stand at a temperature of 30 to 70° C. for 1 to 20 hours. If the aging temperature is less than 30 ℃, there may be a problem that the aging time is too long, leading to an increase in the overall process time, resulting in a decrease in productivity. If the aging temperature is more than 70 ℃, it is out of the boiling point of ethanol, so the solvent by evaporation There may be a problem of increasing the loss of raw materials and increasing the cost of raw materials.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the aging step may be performed in a separate reaction vessel after recovering the silica wet gel blanket having been gelled, or It can be carried out inside the reaction vessel, and in terms of process efficiency and equipment simplification, the aging step can be preferably carried out in the above-described reaction vessel in which gelation has been performed. In addition, when performing the aging step in the reaction vessel in which gelation has been performed, the wet gel blanket composite prepared in step 3) may be rotated, and when aging is performed while rotating, the aging solvent may penetrate better. And, since the dispersion can be made better in the wet gel blanket composite after penetration, there is an advantage that the aging efficiency is greatly improved.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, a solvent replacement step may be performed prior to the drying step for manufacturing an airgel blanket from the wet gel blanket composite. The wet gel of the wet gel blanket composite has pores filled with a solvent including water and/or an organic solvent, and when the solvent is removed by performing the step of drying the wet gel blanket composite, the liquid solvent vaporizes into a gas phase. Shrinkage and cracking of the pore structure occur due to the surface tension of the solvent at the gas/liquid interface. As a result, a decrease in specific surface area and a change in pore structure in the final produced silica airgel occur. Therefore, in order to maintain the pore structure of the wet gel, it is necessary to minimize the surface tension of the solvent, and for this, it is necessary to replace water having high surface tension with a solvent having low surface tension.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, a solvent that can be mixed with silica gel after gelation as the substituted solvent may be a hydrophilic polar organic solvent, and a specific example may be alcohol. Specifically, the alcohol is a monohydric alcohol such as methanol, ethanol, isopropanol, butanol; Alternatively, it may be a polyhydric alcohol such as glycerol, ethylene glycol, propylene glycol, diethylene glycol, dipropylene glycol, and sorbitol, and any one or a mixture of two or more of them may be used. Among these, in consideration of miscibility with water and a hydrophobic airgel, it may be a monohydric alcohol having 1 to 6 carbon atoms such as methanol, ethanol, isopropanol, butanol, and the like.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, a step of drying to manufacture an airgel blanket from the wet gel blanket composite may be performed.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the drying step may be performed through a process of removing the solvent while maintaining the pore structure of the aged gel. Supercritical drying or atmospheric drying process can be used.

In the second aspect of the method for manufacturing the airgel blanket according to an embodiment of the present invention, the supercritical drying process may be performed using supercritical carbon dioxide. Carbon dioxide (CO ₂ ) is in a gaseous state at room temperature and pressure, but when it exceeds the limit of a certain temperature and high pressure called the supercritical point, the evaporation process does not occur, and it becomes a critical state in which gas and liquid cannot be distinguished. Carbon dioxide in the state is called supercritical carbon dioxide. Although supercritical carbon dioxide has a molecular density close to that of a liquid, its viscosity is low, it has a property close to that of a gas, has a fast diffusion, high thermal conductivity, high drying efficiency, and can shorten a drying process time.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, in the supercritical drying process, the wet gel blanket aged in the supercritical drying reactor is put, and then liquid CO ₂ is filled and the wet gel is inside. A solvent replacement process of substituting the alcohol solvent of CO _{2 is performed.} After that, after raising the temperature to 40°C to 70°C at a constant temperature increase rate, specifically at a rate of 0.1°C/min to 1°C/min, a pressure equal to or higher than the pressure at which carbon dioxide becomes a supercritical state, specifically 100 bar to 150 By maintaining the pressure of the bar, the carbon dioxide is maintained for a certain period of time, specifically, 20 minutes to 1 hour in a supercritical state. In general, carbon dioxide becomes supercritical at a temperature of 31 °C and a pressure of 73.8 bar. Carbon dioxide is maintained at a constant temperature and pressure at a supercritical state for 2 to 12 hours, more specifically for 2 to 6 hours, and then the pressure is gradually removed to complete the supercritical drying process to manufacture an airgel blanket. I can.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, in the case of the atmospheric drying process, hot air drying, IR drying, etc. under a temperature and atmospheric pressure (1±0.3 atm) of 70° C. to 200° C. It can be carried out according to a conventional method.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, as a result of the drying process as described above, a blanket including a porous airgel having nano-sized pores may be manufactured. In particular, the silica airgel according to an embodiment of the present invention has excellent physical properties with high hydrophobicity, particularly low density and high porosity, and the silica airgel-containing blanket including the same has low thermal conductivity and excellent mechanical flexibility.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, a compression process for adjusting the thickness before or after the drying process and uniformizing the internal structure and surface shape of the blanket, suitable for use A molding process to have a shape or morphology, or a lamination process of laminating a separate functional layer may be further performed.

The present invention provides an airgel blanket manufacturing apparatus for carrying out the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the airgel blanket manufacturing apparatus includes a bobbin 100 on which a blanket is wound, and the bobbin 100 as shown in FIG. 1. ), a drive member 300 for rotating the bobbin 100 accommodated in the gelling tank 210, and a sol catalyzed by the gelling tank 210 Drying to dry the blanket by raising the temperature of the catalyzed sol supply member 400 for injecting, the aging member for injecting the aging solution into the gelling tank 210 (not shown), and the temperature of the gelling tank 210 Includes members (not shown). Here, the blanket may mean a blanket substrate before the catalyzed sol is introduced, a blanket substrate impregnated with the catalyzed sol, and/or a wet gel blanket after gelation. It can be interpreted appropriately according to.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the bobbin is for winding the blanket in a roll-shape, and a winding rod in which the blanket is wound in a roll shape, and at both ends of the winding rod, respectively It is coupled and includes a support plate for supporting the side of the blanket wound on the winding rod.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the winding rod has a cylindrical shape with a hollow penetrating in the longitudinal direction, and a long sheet-shaped blanket is wound in a roll shape on an outer circumferential surface.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the outside of the blanket wound on the winding rod can quickly impregnate the catalyzed sol, thereby stably gelling, but the inside of the blanket is There is a problem that it takes a lot of time for the catalyzed sol to be impregnated. To prevent this, the outer circumferential surface of the winding rod includes a plurality of connection holes connected to the hollow.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the winding rod has a hollow formed therein so as to introduce the catalyzed sol injected into the gelling tank, and the catalyst is introduced into the hollow. A plurality of connection holes are formed so that the sol flows out of the winding rod and is impregnated into the inside of the blanket wound on the winding rod. Accordingly, the outer and inner sides of the blanket can be gelled by simultaneously impregnating the catalyzed sol, and as a result, the time required for gelling of the blanket can be greatly shortened, and as a result, the entire blanket can be uniformly gelled. .

In the second aspect of the method for manufacturing the airgel blanket according to an embodiment of the present invention, the plurality of connection holes have a diameter of 3 to 5 mm, and are formed at regular intervals on the outer peripheral surface of the winding rod. Accordingly, the sol catalyzed uniformly can be supplied to the entire blanket wound on the outer circumferential surface of the winding rod, and accordingly, the entire inner side of the blanket can be uniformly gelled.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the support plate is to support the blanket wound around the winding rod so that it is not wound irregularly, has a disk shape, and has a disk shape, and is at both ends of the winding rod. It is coupled and supports the side of the blanket wound around the winding rod.

In a second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the support plate includes a fastening groove to which an end of the winding rod is coupled, and a fastening hole formed on a bottom surface of the fastening groove. That is, the support plate may be coupled to the end of the winding rod through the fastening groove.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the support plate has a plurality of open holes, and the plurality of open holes introduces the catalyzed sol to the side of the blanket wound on the winding rod. And thereby stably gelling the side of the blanket.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the bobbin includes a winding rod and a support plate, and accordingly, the blanket can be wound in a roll shape.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the body is provided with a gelling tank accommodating a bobbin, and a gelling tank and a first installation member 220 on which the gelling tank is installed Includes.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the gelling tank is for gelling the blanket accommodated in the bobbin, and is provided inside a gelling chamber for accommodating the bobbin, and is provided at the outer bottom. And an outlet portion connected to the gelation chamber, and an inlet portion provided on the outer upper end and connected to the gelation chamber.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, in particular, in the gelation chamber of the gelation tank, the upper part is opened by a cover, and the lower part has a curvature corresponding to the blanket wound around the winding rod. 'It has a cross-sectional shape, and accordingly, when the silica sol flows into the gelation chamber, the contact force between the silica sol and the blanket can be increased, and as a result, the gelation of the blanket can be increased.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the gelling tank is provided on both walls of the gelling chamber, and the bobbin is rotated in the gelling chamber while being coupled to both ends of the bobbin. It includes a rotating member installed to be possible.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the rotating member is rotatably installed in through-holes formed on both walls of the gelling chamber, and the end of the bobbin accommodated in the gelling chamber is powered It is installed so that it can be delivered.

In a second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, a straight coupling protrusion is formed on one surface of the rotating member, and a straight coupling groove to which the coupling protrusion is coupled to an end of the bobbin is provided. Is formed. That is, the bobbin can be rotated in the same direction when the rotating member is rotated through the coupling of the coupling protrusion and the coupling groove. As a result, the bobbin can be installed rotatably inside the gelation tank.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the main body further includes a second installation member 230 on which a catalyzed sol supply member is installed, and the second installation member is a bottom It includes a piece 231, an installation table 232 installed above the bottom piece and installed so that the catalyzed sol supply member is positioned higher than the gelation tank, and a step 233 installed at one end of the bottom piece.

In a second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the gelling tank includes a rotation handle for rotating the bobbin while being coupled with the other rotation member provided in the gelling tank, and rotation The handle can manually rotate the bobbin from the outside.

In a second aspect of the method for manufacturing the airgel blanket according to an embodiment of the present invention, a maturing member and a drying member are further installed on the mounting table of the second mounting member.

In the second aspect of the method for manufacturing the airgel blanket according to an embodiment of the present invention, the driving member is for rotating the bobbin accommodated in the gelling tank, and power can be transmitted to the other rotating member provided in the gelling tank. Connected to each other. That is, when the driving member rotates the rotating member, the bobbin accommodated in the gelling tank can be rotated in conjunction with the rotating member.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the catalyzed sol supply member is for gelling the blanket by impregnating the blanket wound around the bobbin by injecting silica sol into the gelation tank. It is installed on the mounting table, and the catalyzed sol is supplied to the gelation chamber through the inlet of the gelation tank.

In a second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the aging member is for aging the blanket wound on the bobbin by injecting the aging solution into the gelling tank, and is installed on the mounting table, and the aging solution Is supplied to the gelation chamber through the inlet of the gelation tank.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the drying member is for drying the blanket wound on the bobbin by supplying hot air of high temperature to the gelling tank, and is installed on the mounting table and the gelling tank Dry the blanket contained in the gelation tank by increasing the temperature of

Therefore, the airgel blanket manufacturing apparatus according to the second aspect of the airgel blanket manufacturing method according to an embodiment of the present invention can greatly shorten the manufacturing time of the airgel blanket, and can greatly increase the productivity of the airgel blanket. Blankets can be mass-produced.

In particular, the airgel blanket manufacturing apparatus according to the second aspect of the airgel blanket manufacturing method according to an embodiment of the present invention can induce stable gelation regardless of the thickness and length of the blanket by rotating the blanket, and the bobbin rotates. Therefore, the entire blanket wound around the bobbin can be uniformly gelled, and since only the bobbin rotates without rotating the gelling tank, the shape of the gelling tank is not limited. In addition, as the gelation chamber of the gelation tank is formed in a'U' cross-sectional shape, the blanket wound around the bobbin can be gelled more effectively.

In addition, in the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the airgel blanket manufacturing apparatus includes a bobbin on which a blanket is wound, and the bobbin may include a winding rod and a support plate. have. Here, the outer circumferential surface of the winding rod may include a fixing clip that is inserted and fixed at the winding point of the blanket.

In the second aspect of the method for manufacturing an airgel blanket according to an embodiment of the present invention, the fixing clip has a pin shape having an elastic restoring force, one end is fixed to the outer peripheral surface of the winding rod, and the other end is elastically supported on the outer peripheral surface of the winding rod. . Accordingly, when the starting point of the blanket is inserted between the other end of the fixing clip and the winding rod, the blanket can be fixed to the starting point of the winding rod by the elastic force of the fixing clip, and as a result, the blanket can be easily wound on the outer circumferential surface of the winding rod.

Example

Hereinafter, embodiments of the present invention will be described in detail so that those of ordinary skill in the art can easily implement the present invention. However, the present invention may be implemented in various different forms and is not limited to the embodiments described herein.

Example 1

To the reactor, 31.90 g of prehydrolyzed TEOS (silica content = 20% by weight, HTEOS), 31.35 g of ethanol and 2.8 g of water were added and mixed to prepare a silica precursor composition. In addition, 7.77 g of trimethylethoxysilane (TMES), 47.28 g of ethanol, 4.22 g of water, and 2.75 g of aqueous ammonia (concentration: 30 wt%) were added to another reactor as a hydrophobic agent and mixed to form a catalyst composition. Was prepared. At this time, the amount in the prepared catalyst composition is 5.2 equivalents of total water based on 1 equivalent of TMES, and the base catalyst is 0.64 parts by weight based on 100 parts by weight of the total sol. The prepared silica precursor and the catalyst composition were mixed to prepare a silica sol, and the silica sol was impregnated into a fiber (Glass fiber fiber mat, 10 mm) as a substrate for a blanket. The fibrous composite impregnated with silica sol was left at room temperature for 24 hours to undergo gelation, surface modification, and aging. The prepared silica wet gel blanket was placed in a 7.2 L supercritical extractor and CO ₂ was injected. After that, the temperature in the extractor was raised to 70°C over 1 hour and 20 minutes, and when reaching 70°C and 150 bar, CO ₂ was injected and discharged at a rate of 0.5 L/min for 20 minutes, and the _{injection of CO 2} was stopped for 20 minutes. The process of maintaining was repeated 4 times. When CO2 was injected and discharged, ethanol was recovered through the bottom of the separator. Afterwards, CO ₂ was vented over 2 hours. After the supercritical drying was completed, it was dried at 150° C. and atmospheric pressure for 1 hour to prepare a silica airgel blanket.

Example 2

<Production of catalyzed sol>

A silica precursor composition was prepared by mixing methyltetraethoxysilane (MTES) and tetraethylorthosilicate (TEOS) at a molar ratio of 95:5. The silica precursor composition and water were mixed at a molar ratio of 1:10, and a silica precursor composition and ethanol having a weight ratio of 1:2 were added to prepare a silica sol. Hydrochloric acid was added so that the silica sol had a pH of 3 or less to accelerate hydrolysis. Separately, a 1 vol% ammonia ethanol solution (base catalyst solution) was prepared. The silica sol and the base catalyst solution were mixed in a volume ratio of 9:1 to prepare a catalyzed sol.

<Manufacture of wet gel blanket>

A bobbin wound with 10T (10 mm) glass fiber was fixed to the reaction vessel. The prepared catalyzed sol was put into a reaction vessel, and the bobbin wound around the glass fiber was rotated to perform gelation. At this time, the rate of addition of the catalyzed sol was adjusted so that all of the catalyzed sol could be added before the gelation was completed. When the fiber was sufficiently impregnated and the liquid level in the reaction vessel no longer changed, the remaining sol was recovered by opening the drain valve coupled to the reaction vessel. After 60 minutes, gelation was completed, and aged at a temperature of 60° C. for 20 hours. When the aging was completed, ethanol was added to the reaction vessel at a temperature of 60° C. to replace the solvent.

<Drying process>

Thereafter, the wet gel blanket was placed in a convection oven, and then dried at 150° C. for 2 to 5 hours under normal pressure to completely remove the solvent and moisture to prepare a hydrophobic silica airgel blanket.

Example 3

In Example 2, during the drying process, the wet gel blanket was put into a supercritical extractor, CO ₂ was injected, the temperature in the extractor was raised to 50 °C over 1 hour, and supercritical drying was performed at 50 °C and 100 bar. Thereafter, the same as in Example 2, except that the hydrophobic silica airgel blanket having been completed supercritical drying was dried in an oven at 200° C. for 2 hours at atmospheric pressure to completely remove the solvent and moisture to prepare a hydrophobic silica airgel blanket. It was carried out by the method.

Comparative Example 1

To the reactor, 31.90 g of prehydrolyzed TEOS (HTEOS), 24.41 g of ethanol and 11.12 g of water were added and mixed to prepare a silica precursor composition. In addition, 60.54 g of ethanol and 0.69 g of aqueous ammonia (concentration: 30 wt%) were added to another reactor and mixed to prepare a catalyst composition. The prepared silica precursor and the catalyst composition were mixed to prepare a silica sol, and the silica sol was impregnated into a fiber (Glass fiber fiber mat, 10 mm) as a substrate for a blanket. Gelation was induced for 10 minutes to prepare a silica wet gel blanket. The prepared silica wet gel blanket was aged for 1 hour at a temperature of 50° C. using _{ammonia (NH 3 )/ethanol solution (2.2:97.8 volume ratio).} 90% by volume of a hexamethyldisilazane (HMDS)/ethanol solution (5:95 by volume) based on the volume of the wet gel blanket was added to the aged silica wet gel blanket, and then surface modification was performed at a temperature of 70° C. for 4 hours. .

Thereafter, the wet gel blanket was placed in a convection oven, and then dried at 150° C. for 2 to 5 hours under normal pressure to completely remove the solvent and moisture to prepare a hydrophobic silica airgel blanket.

Comparative Example 2

To the reactor, 31.90 g of prehydrolyzed TEOS (HTEOS), 24.41 g of ethanol and 11.12 g of water were added and mixed to prepare a silica precursor composition. In addition, 60.54 g of ethanol and 0.69 g of aqueous ammonia (concentration: 30 wt%) were added to another reactor and mixed to prepare a catalyst composition. The prepared silica precursor and the catalyst composition were mixed to prepare a silica sol, and the silica sol was impregnated into a fiber (Glass fiber fiber mat, 10 mm) as a substrate for a blanket. Gelation was induced for 10 minutes to prepare a silica wet gel blanket. The prepared silica wet gel blanket was aged for 1 hour at a temperature of 50° C. using _{ammonia (NH 3 )/ethanol solution (2.2:97.8 volume ratio).} 90% by volume of a hexamethyldisilazane (HMDS)/ethanol solution (5:95 by volume) based on the volume of the wet gel blanket was added to the aged silica wet gel blanket, and then surface modification was performed at a temperature of 70° C. for 4 hours. .

Thereafter, the wet gel blanket was placed in a 7.2 L supercritical extractor and CO ₂ was injected. After that, the temperature in the extractor was raised to 70°C over 1 hour and 20 minutes, and when reaching 70°C and 150 bar, CO ₂ was injected and discharged at a rate of 0.5 L/min for 20 minutes, and the _{injection of CO 2} was stopped for 20 minutes. The process of maintaining was repeated 4 times. When CO2 was injected and discharged, ethanol was recovered through the bottom of the separator. Afterwards, CO ₂ was vented over 2 hours. After the supercritical drying was completed, it was dried at 150° C. and atmospheric pressure for 1 hour to prepare a silica airgel blanket.

Comparative Example 3

To the reactor, 31.90 g of prehydrolyzed TEOS (HTEOS), 24.41 g of ethanol and 11.12 g of water were added and mixed to prepare a silica precursor composition. In addition, 60.54 g of ethanol and 0.69 g of aqueous ammonia (concentration: 30 wt%) were added to another reactor and mixed to prepare a catalyst composition. The prepared silica precursor and the catalyst composition were mixed to prepare a silica sol, and the silica sol was impregnated into fibers (Glass fiber fiber mat, 10 mm) as a substrate for a blanket. Gelation was induced for 10 minutes to prepare a silica wet gel blanket. The prepared silica wet gel blanket was aged for 1 hour at a temperature of 50° C. using _{ammonia (NH 3 )/ethanol solution (2.2:97.8 volume ratio).}

After that, the wet gel blanket was placed in a 7.2 L supercritical extractor and CO ₂ was injected. After that, the temperature in the extractor was raised to 70°C over 1 hour and 20 minutes, and when reaching 70°C and 150 bar, CO ₂ was injected and discharged at a rate of 0.5 L/min for 20 minutes, and the _{injection of CO 2} was stopped for 20 minutes. The process of maintaining was repeated 4 times. When CO2 was injected and discharged, ethanol was recovered through the bottom of the separator. Afterwards, CO ₂ was vented over 2 hours. After the supercritical drying was completed, it was dried at 150° C. and atmospheric pressure for 1 hour to prepare a silica airgel blanket.

Comparative Example 4

<Production of catalyzed sol>

A silica sol was prepared by mixing tetraethylorthosilicate (TEOS) and water at a molar ratio of 1:10, and adding TEOS and ethanol having a weight ratio of 1:2. Hydrochloric acid was added so that the silica sol had a pH of 3 or less to accelerate hydrolysis. A silica sol was prepared _{by mixing 0.2 parts by weight of TiO 2 as} an opacifying agent and 0.2 parts by weight of Ultracarb (LKAB) as a flame retardant based on 100 parts by weight of the silica sol and stirring for 30 minutes to prepare a silica sol. Base catalyst solution) was prepared. The silica sol and the base catalyst solution were mixed in a volume ratio of 9:1 to prepare a catalyzed sol.

<Manufacture of wet gel blanket>

A bobbin wound with 10T (10 mm) glass fiber was fixed to the reaction vessel. The prepared catalyzed sol was put into a reaction vessel, and the bobbin wound around the glass fiber was rotated to perform gelation. At this time, the rate of addition of the catalyzed sol was adjusted so that all of the catalyzed sol could be added before the gelation was completed. When the fiber was sufficiently impregnated and the liquid level in the reaction vessel no longer changed, the remaining sol was recovered by opening the drain valve coupled to the reaction vessel. After 30 minutes, when the gelation was completed, the aging solution was added to the reaction vessel, and the bobbin was rotated to proceed with aging. At this time, the aging solution was a 5 vol% ammonia ethanol diluted solution, and was aged for 20 hours at a temperature of 60°C. When the aging was completed, the drain valve was opened to recover the aging solution. Thereafter, the surface modification solution was added to the reaction vessel to perform surface modification while rotating the bobbin, and after completion, the surface modification solution was recovered. At this time, the surface modification solution was a 10 vol% methyltetraethoxysilane (MTES) ethanol diluted solution, and an amount having the same volume ratio as that of the wet gel blanket composite was added. Surface modification (hydrophobicization) was performed at room temperature for 8 hours.

<Drying process>

After that, put the wet gel blanket in a supercritical extractor, CO ₂ was injected, the temperature in the extractor was raised to 50 °C over 1 hour, supercritical drying was performed at 50 °C and 100 bar, and then the hydrophobic supercritical drying was completed. The silica airgel blanket was dried under normal pressure in an oven at 200° C. for 2 hours to completely remove residual salt and moisture to prepare a hydrophobic silica airgel blanket.

Experimental example

For the silica airgel blankets prepared in Examples 1 to 3 and Comparative Examples 1 to 4, the moisture impregnation rate of 28 days (MIR-28D), the moisture impregnation rate of 96 hours (MIR-96H), and moisture impregnation of 15 minutes The rate (MIR-15M), dust generation amount, and room temperature thermal conductivity were measured as follows and are shown in Tables 1 and 2, respectively.

* Moisture impregnation rate of 28 days (MIR-28D, wt%): With respect to the silica airgel blanket prepared in each Example and Comparative Example, a 100 mm x 100 mm size specimen was floated on distilled water at 21 ± 2 °C, and A 6.4 mm mesh screen was raised and soaked to 127 mm below the water surface and impregnated. After 28 days, the mesh screen was removed, and when the specimen emerged, the specimen was picked up with a clamp and suspended vertically for 60 ± 5 seconds. Thereafter, the weight before and after impregnation was measured to check the weight increase rate, and the moisture impregnation rate of 28 days was calculated using Equation 1 below. The lower the moisture impregnation rate on 28 days, the higher the long-term water repellency of the airgel blanket.

[Equation 1]

Moisture impregnation rate at 28 days (MIR-28D, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2 ℃ for 28 days-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100

* Moisture impregnation rate of 96 hours (MIR-96H, wt%): With respect to the silica airgel blanket prepared in each Example and Comparative Example, a 100 mm x 100 mm size specimen was floated on distilled water at 21±2° C. on the specimen. A 6.4 mm mesh screen was raised and soaked to 127 mm below the water surface and impregnated. After 96 hours, the mesh screen was removed, and when the specimen floated, the specimen was picked up with a clamp and suspended vertically for 60 ± 5 seconds. Thereafter, the weight before and after the impregnation was measured to check the weight increase rate, and the moisture impregnation rate of 96 hours was calculated using Equation 2 below. The lower the 96-hour moisture impregnation rate indicates that the airgel blanket has a higher medium-term water repellency.

[Equation 2]

Moisture impregnation rate of 96 hours (MIR-96H, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2℃ for 96 hours-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100

* Moisture impregnation rate of 15 minutes (MIR-15M, wt%): With respect to the silica airgel blanket prepared in each Example and Comparative Example, a 100 mm x 100 mm size specimen was floated on distilled water at 21±2° C. on the specimen. A 6.4 mm mesh screen was raised and soaked to 127 mm below the water surface and impregnated. After 15 minutes, the mesh screen was removed, and when the specimen floated, the specimen was picked up with a clamp and suspended vertically for 60 ± 5 seconds. Thereafter, the weight before and after impregnation was measured to check the weight increase rate, and the moisture impregnation rate of 15 minutes was calculated using Equation 3 below. The lower the moisture impregnation rate of 15 minutes, the higher the short-term water repellency of the airgel blanket.

[Equation 3]

Moisture impregnation rate of 15 minutes (MIR-15M, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2 ℃ for 15 minutes-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100

* Dust generation amount (% by weight): With respect to the silica airgel blanket prepared in each Example and Comparative Example, a 12 mm x 12 mm size specimen was subjected to vibration for 6 hours under a vibration condition of 18 Hz/6 mm. Thereafter, the weight before and after the vibration was measured to check the weight reduction rate, and the amount of dust generated was calculated using Equation 10 below. The lower the amount of dust generated, the better the workability.

[Equation 10]

Dust generation amount (% by weight) = {(weight of airgel blanket before vibration-weight of airgel blanket after vibration of 18 Hz/6mm)/weight of airgel blanket before vibration generation} X 100

* Room temperature thermal conductivity (mW/mK): Prepare a sample having a size of 30 cm X 30 cm in the silica airgel blanket prepared in each Example and Comparative Example, and use the HFM 436 Lambda equipment of NETZSCH for the sample at room temperature (23±5° C.) The thermal conductivity was measured.

division Example One 2 3 Silica sol ¹⁾ (Kinds) TMES:TEOS MTES:TEOS MTES:TEOS (Molar ratio) 38:62 95:5 95:5 Surface modification step X X X Drying step Supercritical Normal pressure Supercritical 15 minutes moisture impregnation rate (weight%) 1.5 1.2 1.0 96 hours moisture impregnation rate (weight%) 40.0 10.0 9.0 Water impregnation rate of 28 days (weight%) 50.0 25.0 23.0 (MIR-28D)-(MIR-15M) 48.5 23.8 22.0 Dust generation amount (weight%) 0.3 0.4 0.3 Room temperature thermal conductivity (mW/mK) 19.5 19.5 19.2 1) a silicate containing a hydrophobic agent or a hydrophobic group in a silica sol: a silica precursor

division Comparative example One 2 3 4 Silica sol ²⁾ (Kinds) TEOS TEOS TEOS TEOS (Molar ratio) 100 100 100 100 Surface modification step O
(HMDS) O
(HMDS) X O
(MTES) Drying step Normal pressure Supercritical Supercritical Supercritical 15 minutes moisture impregnation rate (weight%) 4.0 1.4 X 10.0 96 hours moisture impregnation rate (weight%) 60.0 55.0 X 75.0 Water impregnation rate of 28 days (weight%) 102.0 103.0 X 110.0 (MIR-28D)-(MIR-15M) 98.0 101.6 X 100.0 Dust generation amount (weight%) 1.6 0.3 0.8 0.5 Room temperature thermal conductivity (mW/mK) 28.5 19.1 23.4 21.0 2) silica precursor in silica sol

As shown in Tables 1 and 2, in the case of Example 1 carried out according to the first aspect of the method for manufacturing an airgel blanket of the present invention, it was confirmed that short-term water repellency as well as mid-term water repellency and long-term water repellency were excellent. , In the case of Examples 2 and 3 carried out according to the second aspect of the airgel blanket manufacturing method of the present invention, it was confirmed that short-term water repellency, medium-term water repellency, and long-term water repellency were excellent regardless of drying conditions. This is due to the fact that in the airgel blanket manufactured according to the present invention, a hydrophobic group is uniformly introduced not only to the outermost surface of the airgel, but also to the inner surface of the airgel.

Further, it was confirmed that all of Examples 1 to 3 according to the present invention have excellent dust generation and room temperature thermal conductivity.

On the other hand, unlike the first and second aspects of the method for manufacturing an airgel blanket of the present invention, when preparing the silica sol, only the silica precursor was alone and the surface was modified from a separate surface modification step. It was confirmed that both short-term and mid-term water repellency as well as water repellency were poor, and dust generation and room temperature thermal conductivity were also increased compared to the examples.

In addition, in the case of Comparative Example 2 in which supercritical drying was performed under the drying conditions compared to Comparative Example 1, the short-term water repellency seemed to be improved compared to Comparative Example 1, but it was confirmed that the long-term water repellency was not improved. This is because even if the surface modification step is additionally performed, a sufficient amount of the surface modifier is not introduced into the interior of the airgel, so when the airgel is exposed to moisture for a long time regardless of the drying conditions, moisture infiltrates the interior of the aerogel and the surface inside the airgel. This is due to the fact that moisture adsorption occurred by hydrogen bonding between the hydroxyl group present in and moisture.

In addition, unlike the first and second aspects of the method for manufacturing an airgel blanket of the present invention, when preparing the silica sol, in the case of Comparative Example 3, in which only the silica precursor was alone and no separate surface modification step was performed, the airgel blanket It was confirmed that the moisture was impregnated in a very excessive amount so that the moisture impregnation rate could not be measured due to its own hydrophilicity, and the room temperature thermal conductivity was also increased compared to the examples.

In addition, in the case of Comparative Example 4 in which the silicate containing a hydrophobic group according to the second aspect of the method for manufacturing an airgel blanket of the present invention was not included in the silica precursor composition, but was used as a surface modifier in the surface modification step in the same amount, the surface modifier was It was confirmed that short-term water repellency, medium-term water repellency, and long-term water repellency were all poor because the function as a hydrophobic agent was not sufficient, and a sufficient amount of surface modifier was not introduced into the airgel.

From these results, it was confirmed that the airgel blanket according to the present invention has excellent long-term water repellency, so that the thermal insulation performance of the airgel blanket can be maintained even under severe conditions that may be exposed to moisture for a long time.

The above description of the present invention is for illustrative purposes only, and those of ordinary skill in the art to which the present invention pertains will be able to understand that other specific forms can be easily modified without changing the technical spirit or essential features of the present invention. will be. Therefore, it should be understood that the embodiments described above are illustrative and non-limiting in all respects.

100: bobbin 110: winding rod
120: support plate 200: main body
210: gelation tank 212: discharge unit
213: inlet 214: cover
215: rotating member 216: rotating handle
220: first installation member 230: second installation member
231: bottom part 232: mounting table
233: stairs 300: driving member
400: catalyzed sol supply member

Claims (10)

An airgel blanket having a moisture impregnation rate (MIR-28D) of 100% by weight or less on 28 days calculated by the following Equation 1:
[Equation 1]
Water impregnation rate of 28 days (MIR-28D, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2°C for 28 days-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100. The method of claim 1,
The airgel blanket that the moisture impregnation rate of 28 days (MIR-28D) calculated by Equation 1 and the moisture impregnation rate of 15 minutes (MIR-15M) calculated by Equation 3 below satisfies Equation 4:
[Equation 3]
Moisture impregnation rate of 15 minutes (MIR-15M, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2 ℃ for 15 minutes-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100
[Equation 4]
(MIR-28D)-(MIR-15M) ≤ 100. The method of claim 1,
The airgel blanket that the moisture impregnation rate of 28 days calculated by Equation 1 (MIR-28D) and the moisture impregnation rate of 15 minutes (MIR-15M) calculated by Equation 3 below satisfy Equation 5:
[Equation 3]
Moisture impregnation rate of 15 minutes (MIR-15M, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2 ℃ for 15 minutes-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100
[Equation 5]
1 ≤ (MIR-28D)-(MIR-15M) ≤ 90. The method of claim 1,
The airgel blanket having a moisture impregnation rate (MIR-28D) of 70% by weight or less on 28 days calculated by Equation 1 above. The method of claim 1,
The airgel blanket is an airgel blanket having a moisture impregnation rate of 15 minutes (MIR-15M) calculated by Equation 3 below of 20% by weight or less:
[Equation 3]
Moisture impregnation rate of 15 minutes (MIR-15M, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2℃ for 15 minutes-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100. The method of claim 1,
The airgel blanket is an airgel blanket having a moisture impregnation rate (MIR-96H) of 50% by weight or less for 96 hours calculated by the following equation:
[Equation 2]
Moisture impregnation rate of 96 hours (MIR-96H, wt%) = {(weight of airgel blanket after immersion in distilled water at 21±2°C for 96 hours-weight of airgel blanket before impregnation with distilled water)/weight of airgel blanket before impregnation with distilled water} X 100. The method of claim 1,
The airgel blanket is an airgel blanket having a dust generation amount of 3.0% by weight or less calculated by the following Equation 10:
[Equation 10]
Dust generation amount (% by weight) = {(weight of airgel blanket before vibration-weight of airgel blanket after vibration of 18 Hz/6mm)/weight of airgel blanket before vibration occurrence} X 100. The method of claim 1,
The airgel blanket is an airgel blanket having a thermal conductivity of 30.0 mW/mK or less at room temperature (23±5° C.). The method of claim 1,
The airgel blanket includes an airgel and a substrate for a blanket,
The airgel blanket in which the airgel is formed inside and on the surface of the substrate for the blanket. The method of claim 9,
The airgel blanket is that the airgel includes a hydrophobic group on the inner surface of the airgel.

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